In vitro assessment of the bioaccessibility of brominated flame retardants in indoor dust using a colon extended model of the human gastrointestinal tract

An in vitro colon extended physiologically based extraction test (CEPBET) which incorporates human gastrointestinal tract (GIT) parameters (including pH and chemistry, solid-to-fluid ratio, mixing and emptying rates) was applied for the first time to study the bioaccessibility of brominated flame retardants (BFRs) from the 3 main GIT compartments (stomach, small intestine and colon) following ingestion of indoor dust. Results revealed the bioaccessibility of γ-HBCD (72%) was less than that for α- and β-isomers (92% and 80% respectively) which may be attributed to the lower aqueous solubility of the γ-isomer (2 μg L−1) compared to the α- and β-isomers (45 and 15 μg L−1 respectively). No significant change in the enantiomeric fractions of HBCDs was observed in any of the studied samples. However, this does not completely exclude the possibility of in vivo enantioselective absorption of HBCDs, as the GIT cell lining and bacterial flora – which may act enantioselectively – are not included in the current CE-PBET model. While TBBP-A was almost completely (94%) bioaccessible, BDE-209 was the least (14%) bioaccessible of the studied BFRs. Bioaccessibility of tri-hepta BDEs ranged from 32–58%. No decrease in the bioaccessibility with increasing level of bromination was observed in the studied PBDEs.

Peat as a natural solid-phase for copper preconcentration and determination in a multicommuted flow system coupled to flame atomic absorption spectrometry

The physical and chemical characteristics of peat were assessed through measurement of pH, percentage of organic matter, cationic exchange capacity (CEC), elemental analysis, infrared spectroscopy and quantitative analysis of metals by ICP OES. Despite the material showed to be very acid in view of the percentage of organic matter, its CEC was significant, showing potential for retention of metal ions. This characteristic was exploited by coupling a peat mini-column to a flow system based on the multicommutation approach for the in-line copper concentration prior to flame atomic absorption spectrometric determination. Cu(II) ions were adsorbed at pH 4.5 and eluted with 0.50 mol L(-1) HNO(3). The influence of chemical and hydrodynamic parameters, such as sample pH, buffer concentration, eluent type and concentration, sample flow-rate and preconcentration time were investigated. Under the optimized conditions, a linear response was observed between 16 and 100 mu g L(-1), with a detection limit estimated as 3 mu g L(-1) at the 99.7% confidence level and an enrichment factor of 16. The relative standard deviation was estimated as 3.3% (n = 20). The mini-column was used for at least 100 sampling cycles without significant variation in the analytical response. Recoveries from copper spiked to lake water or groundwater as well as concentrates used in hemodialysis were in the 97.3-111 % range. The results obtained for copper determination in these samples agreed with those achieved by graphite furnace atomic absorption spectrometry (GFAAS) at the 95% confidence level. (C) 2009 Elsevier B.V. All rights reserved.

Thermal analysis of an enriched flame incinerator for aqueous residues

The use of oxygen to enrich the combustion air can be an attractive technique to increase capacity of an incinerator originally designed to operate with air, If incinerator parameters such as operation temperature, turbulence level and residence time are fixed for a certain fuel supply rate, it is possible to increase the residue consumption rate using enriched air. This paper presents the thermal analysis for operation with enriched air of an aqueous residue experimental incinerator. The auxiliary fuel was diesel oil. The theoretical results showed that there is a considerable increase in the incineration ratio up to approximately 50% of O-2 in the oxidiser. The tendency was confirmed experimentally. Thermal analysis was demonstrated to be an important tool to predict possible incinerator capacity increase. (C) 2005 Published by Elsevier Ltd.

Properties of DLC films deposited by an oxyacetylene flame

Diamond-like carbon (DLC) films were obtained by spinning a tungsten carbide substrate at a high speed using an oxyacetylene flame. The films deposited at a typical experimental condition of substrate temperature of 810 degrees C, rotation of 600 rpm and 3 h deposition time, exhibited an uniform, very smooth, hard and glassy surface covering the entire exposed face of the substrate. These films were identified as DLC by their characteristic broad Raman spectra centered at 1554 cm(-1) and micro-Vicker's hardness > 3400 kg mm(-2). For substrate temperatures < 800 degrees C the film started losing the uniform glassy surface and the hardness deteriorated. For temperatures > 950 degrees C the film was still hard and shiny, but black in color. DLC films were also obtained in a wide range of speeds of rotation (300-750 rpm), as long as the temperature remained close to 850 degrees C. (C) 1999 Elsevier B.V. S.A. All rights reserved.

Application of cellulose modified with p-aminobenzoic groups in preconcentration system for determination of Cu, Fe, Ni, and Zn in fuel ethanol samples by flame atomic absorption spectrometry

Cellulose chemically modified with p-aminobenzoic groups, abbreviated as Cel-PAB, was used for preconcentration of copper, iron, nickel, and zinc from ethanol fuel, normally used in Brazil as engine fuel. The surface characteristics and the surface area of the cellulose were obtained before and after chemical modification using FT-IR, elemental analysis, and surface area analysis (B.E.T.). The retention and recovery of the analyte elements were studied by applying batch and column techniques.

Flame AAS determination of metal ions in fuel ethanol after preconcentration on acid carboxymethylcellulose (CMCH)

This paper describes the preparation of acid carboxymethylcellulose (CMCH), and the results of a study on the adsorption and preconcentration (using batch and flow-through column methods) of Cd(II), Cu(II), Cr(III), Fe(III), Ni(II) and Zn(II) in ethanol medium. The adsorption capacities for each metallic ion were (in mmol g(-1)) Cd(II) = 0.92; Cu(II) = 1.45; Cr(III) = 1.70; Fe(III) = 1.60; Ni(II) = 1.30; and Zn(II) = 1.10. By means of the flow-through method, a recovery of ca. 100% of the metallic ions adsorbed in a column packed with 2 g of CMCH was found when 5.0 mL of 1.0 mol L-1 hydrochloric acid were used as eluent. An enrichment factor of 20 (100 mt solution containing 50 mu g L-1 of the metallic ions, concentrated to 5.0 mt) was obtained by this preconcentration procedure. The sorption-desorption procedure applied allowed the development of a preconcentration and Flame AAS quantification method of metallic ions in fuel ethanol at trace levels.

Determination of metal ions in natural waters by flame-AAS after preconcentration on a 5-amino-1,3,4-thiadiazole-2-thiol modified silica gel.

5-amino-1,3,4-thiadiazole-2-thiol groups attached on a silica gel surface have been used for adsorption of Cd(II), Co(II), Cu(II), Fe(III), Ni(II), Pb(II) and Zn(II) from aqueous solutions. The adsorption capacities for each metal ion were (in mmol.g(-1)): Cd(II)= 0.35, Co(II)= 0.10, Cu(II)= 0.15, Fe(III)= 0.20, Hg(Il)= 0.46, Ni(II)= 0.16, Pb(II)= 0.13 and Zn(II)= 0.15. The modified silica gel was applied in the preconcentration and quantification of trace level metal ions present in water samples (river, and bog water).

WC-CoCr coatings sprayed by high velocity oxygen-fuel (HVOF) flame on AA7050 aluminum alloy: electrochemical behavior in 3.5% NaCl solution

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Mathematical equation correction to spectral and transport interferences in high-resolution continuum source flame atomic absorption spectrometry: determination of lead in phosphoric acid

Um método de correção de interferência espectral e de transporte é proposto, e foi aplicado para minimizar interferências por moléculas de PO produzidas em chama ar-acetileno e de transporte causada pela variação da concentração de ácido fosfórico. Átomos de Pb e moléculas de PO absorvem a 217,0005 nm, então Atotal217,0005 nm = A Pb217,0005 nm + A PO217,0005 nm. Monitorando o comprimento de onda alternativo de PO em 217,0458 nm, é possível calcular a contribuição relativa de PO na absorbância total a 217,0005 nm: A Pb217,0005 nm = Atotal217,0005 nm - A PO217,0005 nm = Atotal217,0005 nm - k (A PO217,0458 nm). O fator de correção k é a razão entre os coeficientes angulares de duas curvas analíticas para P obtidas a 217,0005 e 217,0458 nm (k = b217,0005 nm/b217,0458 nm). Fixando-se a taxa de aspiração da amostra em 5,0 ml min-1, e integrando-se a absorbância no comprimento de onda a 3 pixels, curvas analíticas para Pb (0,1 - 1,0 mg L-1) foram obtidas com coeficientes de correlação típicos > 0,9990. As correlações lineares entre absorbância e concentração de P nos comprimentos de onda 217,0005 e 217,0458 foram > 0,998. O limite de detecção de Pb foi 10 µg L-1. O método de correção proposto forneceu desvios padrão relativos (n=12) de 2,0 a 6,0%, ligeiramente menores que os obtidos sem correção (1,4-4,3%). As recuperações de Pb adicionado às amostras de ácido fosfórico variaram de 97,5 a 100% (com correção pelo método proposto) e de 105 a 230% (sem correção).

Fast sequential multi-element determination of Ca, Mg, K, Cu, Fe, Mn and Zn for foliar diagnosis using high-resolution continuum source flame atomic absorption spectrometry: Feasibility of secondary lines, side pixel registration and least-squares background correction

The fast sequential multi-element determination of Ca, Mg, K, Cu, Fe, Mn and Zn in plant tissues by high-resolution continuum source flame atomic absorption spectrometry is proposed. For this, the main lines for Cu (324.754 nm), Fe (248.327 nm), Mn (279.482 nm) and Zn (213.857 nm) were selected, and the secondary lines for Ca (239.856 nm), Mg (202.582 nm) and K (404.414 nm) were evaluated. The side pixel registration approach was studied to reduce sensitivity and extend the linear working range for Mg by measuring at wings (202.576 nm; 202.577 nm; 202.578 nm; 202.580 nm: 202.585 nm; 202.586 nm: 202.587 nm; 202.588 nm) of the secondary line. The interference caused by NO bands on Zn at 213.857 nm was removed using the least-squares background correction. Using the main lines for Cu, Fe, Mn and Zn, secondary lines for Ca and K, and line wing at 202.588 nm for Mg, and 5 mL min(-1) sample flow-rate, calibration curves in the 0.1-0.5 mg L-1 Cu, 0.5-4.0 mg L-1 Fe, 0.5-4.0 mg L-1 Mn, 0.2-1.0 mg L-1 Zn, 10.0-100.0 mg L-1 Ca, 5.0-40.0 mg L-1 Mg and 50.0-250.0 mg L-1 K ranges were consistently obtained. Accuracy and precision were evaluated after analysis of five plant standard reference materials. Results were in agreement at a 95% confidence level (paired t-test) with certified values. The proposed method was applied to digests of sugar-cane leaves and results were close to those obtained by line-source flame atomic absorption spectrometry. Recoveries of Ca, Mg, K, Cu, Fe, Mn and Zn in the 89-103%, 84-107%, 87-103%, 85-105%, 92-106%, 91-114%, 96-114% intervals, respectively, were obtained. The limits of detection were 0.6 mg L-1 Ca, 0.4 mg L-1 Mg, 0.4 mg L-1 K, 7.7 mu g L-1 Cu, 7.7 mu g L-1 Fe, 1.5 mu g L-1 Mn and 5.9 mu g L-1 Zn. (C) 2009 Elsevier B.V. All rights reserved.

Determination of macro- and micronutrients in plant leaves by high-resolution continuum source flame atomic absorption spectrometry combining instrumental and sample preparation strategies

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Determination of Zinc in Lubricating Oil by Flame MS Employing Ultrasonic Extraction

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Evaluation of alternate lines of Fe for sequential multi-element determination of Cu, Fe, Mn and Zn in soil extracts by high-resolution continuum source flame atomic absorption spectrometry

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

DETERMINATION of SILICON IN LUBRICANT OIL BY HIGH-RESOLUTION CONTINUUM SOURCE FLAME ATOMIC ABSORPTION SPECTROMETRY USING LEAST-SQUARE BACKGROUND CORRECTION and INTERNAL STANDARDIZATION

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Internal standardization and least-squares background correction in high-resolution continuum source flame atomic absorption spectrometry to eliminate interferences on determination of Pb in phosphoric acid

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)